SYNTHESIS AND PILLARING OF A LAYERED VANADIUM-OXIDE FROM V2O5 AT AMBIENT-TEMPERATURE

The synthesis and structural characterization of an amine-intercalated layered vanadium oxide and its silica-pillared derivative are describ ed. The amine-intercalated vanadium oxide was prepared by reacting V2O 5 with a mixture of alkylamine and a small amount of water at ambient temperature. The layer structure was examined by means of various anal ytical techniques, such as X-ray powder diffraction, thermal analysis, IR, W-Vis and NMR spectroscopy, as well as elemental analysis. The al kylammonium ion-formed bilayers in the interlayer were ion-exchangeabl e with alkali ions. Moreover, ESR spectra showed that vanadium retaine d pentavalence through the intercalation reaction, although a small po rtion of vanadium was found to be reduced after the compound was store d in air for longer than 24 h. By reacting the amine-intercalated laye r vanadia with a solution of tetraethyl orthosilicate, amine and aceto ne, followed by calcination, a silica-pillared derivative of microporo us structure and high surface area was obtained. (C) 1998 Elsevier Sci ence B.V. All rights reserved.